KR920002411B1 - Coating method on selected surface areas by a vacuum evaporation - Google Patents

Coating method on selected surface areas by a vacuum evaporation Download PDF

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KR920002411B1
KR920002411B1 KR1019890019870A KR890019870A KR920002411B1 KR 920002411 B1 KR920002411 B1 KR 920002411B1 KR 1019890019870 A KR1019890019870 A KR 1019890019870A KR 890019870 A KR890019870 A KR 890019870A KR 920002411 B1 KR920002411 B1 KR 920002411B1
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plating
vacuum
concealment
partially
colors
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KR910012331A (en
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곽철남
정천구
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삼성시계주식회사
김정상
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/46—Sputtering by ion beam produced by an external ion source

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

electrolyte-plating nickel (Ni), chromium (Cr), cadmium (Cd), copper (Cu), indium (In), cobalt (Co), silver (Ag), gold (Ag), palladium (Pd) and an alloy of these on a pure metal or metallic alloy; coating a portion with a hiding material; vacuum-plating and then peeling the hiding mterial, so that two color is generated. Duplicate plating by the method (vacuum plating, electrolyte plating or electolyte free plating) and peeling the hiding material, so that three color is generated.

Description

진공도금을 이용한 부분도금 방법Partial Plating Method Using Vacuum Plating

제1도는 종래의 진공도금의 예시도로서 제1a도는 아크방전형 이온 플레이팅 방식의 예시도이고, 제1b도는 스퍼터(SPUTTER)방식의 예시도이다.FIG. 1 is an exemplary view of a conventional vacuum plating, in which FIG. 1a is an illustration of an arc discharge ion plating method, and FIG. 1b is an illustration of a sputter method.

제2도는 본 발명의 표면처리법에 의해 얻어진 표면처리층의 단면을 나타낸 것이다.2 shows a cross section of the surface treatment layer obtained by the surface treatment method of the present invention.

본 발명은 진공도금을 이용한 부분도금 방법에 관한 것이다.The present invention relates to a partial plating method using vacuum plating.

더욱 특별하게는, 본 발명은 PVD(PHYSICAL VAPOR DEPOSITION)법에 의한 진공도금, 또는 진공도금과 습식도금의 조합으로 금색, 은색, 흑색등의 부드럽고 미려한 막을 이중, 삼중코팅하여 부분도금의 최종피막을 수득하는 방법에 관한 것이다.More specifically, the present invention provides a final coating of partial plating by double and triple coating of soft, beautiful films such as gold, silver, and black by vacuum plating by PVD (PHYSICAL VAPOR DEPOSITION) method or a combination of vacuum plating and wet plating. It relates to a method of obtaining.

일반적으로 진공도금 방법은 크게 PVD(PHYSICAL VAPOR DEPOSITION) 방식과 CVD(CHEMICAL VAPOR DEPOSITION)방식으로 구분되며, 이중 PVD 방법은 비교적 간단하고 효율적이라는 점에서 널리 사용되고 있다. 이러한 PVD 방식은 다시 진공도금 내부의 처리방법에 따라 진공증착, 이온플레이팅, 스퍼터링 방법으로 구분될 수 있다.In general, the vacuum plating method is largely divided into PVD (PHYSICAL VAPOR DEPOSITION) method and CVD (CHEMICAL VAPOR DEPOSITION) method, and the double PVD method is widely used in that it is relatively simple and efficient. The PVD method may be further classified into vacuum deposition, ion plating, and sputtering methods according to the processing method inside the vacuum plating.

아크방전 타입의 이온플레이팅 방법은 제1a도에 나타낸 바와같이 진공조내에 증발원 이온화전극, 기판차폐판을 설치하고 증발물에 따른 열전자 방사용 전극을 설치하며, 진공조내에 증발원 이온화전극, 기판차폐판을 설치하고 증발물에 따른 열전자 방사용 전극을 설치하며, 진공조에는 1×10-3-1×10-5PA(10-5-10-7TORR)의 고진공으로 배기하고 전자빔에 의해 증발재를 증발시켜 GAS와의 조합에 의해 막을 형성하는 도금방식이다.In the arc discharge type ion plating method, as shown in FIG. 1A, an evaporation source ionization electrode and a substrate shielding plate are installed in a vacuum chamber, and a thermoelectron emission electrode is installed according to the evaporation material. Install the plate and install the electrode for the thermoelectron emission according to the evaporate, and evacuate the vacuum chamber with high vacuum of 1 × 10 -3 -1 × 10 -5 PA (10 -5 -10 -7 TORR) and evaporate by electron beam It is a plating method in which ash is evaporated to form a film by combination with GAS.

그리고 스퍼터링방식은 제1b도에 나타난 바와 같이 아르곤과 같은 불활성 가스를 극소량 진공조내에 주입하면 진공내에서는 타겟트(TARGET)와 증착할 제품을 포함하고 있어 타겟트에 불활성 가스가 충돌하여 타겟트 분자가 튀어나오고 전자를 방출하게 되어 이것들이 프라스마지대를 형성시키게 되며 이때 +이온을 외부전원 및 타겟트등과의 충돌에 의해 가속되며, 타겟트 등과의 충돌에 의해 가소되며, 타겟트 분자는 충돌이온과 거의 같은 수준의 에너지로 파도금물에 높은 밀착력을 갖는 막을 형성하는 방법이다.As shown in FIG. 1B, the sputtering method includes a target (TARGET) and a product to be deposited in a vacuum when an inert gas such as argon is injected into a vacuum chamber, and the target molecule collides with the target inert gas. Is emitted and electrons are emitted to form a plasma zone, where + ions are accelerated by collision with an external power source and target, and are plasticized by collision with a target. It is a method of forming a film having high adhesion to wave cracking with almost the same level of energy.

그러나 이와같은 종래의 진공도금방법은 대략 금색, 은색, 흑색, 브라운색의 단일색상의 고경도막을 형성하는데 국한된다. 따라서 시계, 안경태, 장식품, 기타제품의 다양화된 패션모델이 요구되는 현싯점에서는 많은 제약과 문제점이 따른다.However, such a conventional vacuum plating method is limited to forming a high hardness film of a single color of about gold, silver, black and brown. Therefore, there are many restrictions and problems in the present situation where diversified fashion models of watches, eyeglasses, ornaments, and other products are required.

본 발명자들은 종래에는 단일색상도금에만 국한되었던 진공도금 방법을 사용하는 부분도금방법을 개발하고, 본 발명을 완성하게 되었다.The present inventors have developed a partial plating method using a vacuum plating method, which was conventionally limited to single color plating, and completed the present invention.

본 발명의 목적은 뛰어난 외관색상, 도금의 지속성, 변색방지 및 표면성질변화등 우수한 특성을 나타낼 수 있는 고경도 진공도금을 이용한 부분도금 방법을 제공하는 것이다.SUMMARY OF THE INVENTION An object of the present invention is to provide a partial plating method using high hardness vacuum plating that can exhibit excellent appearance color, durability of plating, discoloration prevention and surface property change.

본 발명의 또다른 목적은 불가능한 것으로 여겨왔던 전해도금(또 다른 무전해도금)과의 부분도금을 실시함으로서 화려한 이중, 삼중, 색상을 도출할 수 있는 부분도금 방법을 제공하는 것이다.It is another object of the present invention to provide a partial plating method that can derive brilliant double, triple, and color by performing partial plating with electroplating (another electroless plating) which has been considered impossible.

본 발명의 방법을 순금속 혹은 금속합금을 전해 또는 무전해 방법진공방법으로 도금하여 금속의 새로운층을 형성시키고, 이 새로운 층이나 고진공층위에 피막을 보호하기 위한 은폐물을 부분적으로 형성시키고, 진공상태에서 피도금체를 놓고 진공도금을 실시한후, 은폐물을 박리하여 부분도금하는 것이다.The method of the present invention is plated with a pure metal or metal alloy by an electrolytic or electroless method vacuum method to form a new layer of metal, partially forming a concealment on the new layer or high vacuum layer to protect the film, and in a vacuum state. After placing the object to be plated and performing vacuum plating, the concealment is peeled off and partially plated.

전해 또는 무전해 도금방법은 이 분야에서 통상적으로 사용되는 도금방법을 이용한다. 전해 또는 무전해 도금하는 금속으로는 니켈, 크롬, 팔라듐, 로듐, 금, 은, 카드뮴, 구리, 인듐, 코발트 및 이들의 합금이 사용될 수 있다.Electrolytic or electroless plating method uses a plating method commonly used in this field. Nickel, chromium, palladium, rhodium, gold, silver, cadmium, copper, indium, cobalt and alloys thereof may be used as the metal to be electrolytically or electroless plated.

피막을 보호하기 위한 은폐물은 잉크류, 도료류등이며, 내열성, 내약품성, 내분위기성, 및 내박리성이 있는 것이어야 한다.The concealment for protecting the film is ink, paint, etc., and should be heat resistant, chemical resistant, atmosphere resistant, and peelable.

본 발명의 방법의 보다 구체적인 예를들면, 순금속 또는 금속합금상에 니켈, 크륨, 팔라듐, 로듐, 금, 은, 카드뮴, 구리, 인듐, 코발트 또는 그 합금의 전해 도금을 실시하고, 은폐물로 부분도포한후, 진공도금을 실시하고 은폐물을 박리시킴으로써 2색을 나타낼 수 있다. 또한 순금속 또는 금속합금상에 진공도금을 실시하고, 은폐물로 부분도포한후, 니켈, 크롬, 팔라듐, 로듐, 금, 은, 카드뮴, 구리, 인듐, 코발트 또는 그 합금의 전해 도금 또는 무전해도금을 실시하고 은폐물을 박리하여 2색을 나타낼 수 있다.More specific examples of the method of the present invention include electrolytic plating of nickel, chromium, palladium, rhodium, gold, silver, cadmium, copper, indium, cobalt or alloys thereof on a pure metal or metal alloy, and partially coated with a concealment. After that, two colors can be obtained by performing vacuum plating and peeling off the concealed substance. In addition, vacuum plating is performed on pure metals or metal alloys, and partially coated with concealed materials, and then electroplating or electroless plating of nickel, chromium, palladium, rhodium, gold, silver, cadmium, copper, indium, cobalt or alloys thereof. And concealment can be peeled off to give two colors.

또다른 방법으로는 순금속, 또는 합금상에 Ti, Tin, TiCN 막층을 진공도금하고, 이 상부에 은폐물을 부분도포한후 다시 진공도금을 실시한후에 은폐물을 박리하여 2색을 나타내는 방법이 있다.Another method is to vacuum-plat a Ti, Tin, TiCN film layer on a pure metal or alloy, partially coat the concealment on the upper part, and vacuum-plating again, and then peel off the concealment to give two colors.

상기와 같은 본 발명의 방법들을 중복실시하고 은폐물을 박리하여 3색이상을 나타내게 할수도 있다. 하기의 실시예 및 실험예는 본 발명을 더욱 상세히 설명하는 것이며 이들 실시예에 의해 본 발명이 제한되는 것은 아니다.The method of the present invention as described above may be repeated and the concealed material may be peeled off to display three or more colors. The following Examples and Experimental Examples illustrate the present invention in more detail, and the present invention is not limited to these examples.

[실시예]EXAMPLE

제2a도는 본 발명의 처리법에 의해 얻어진 표면처리층의 단면을 나타낸 것이다. 소재 1은 SUS 및 BSP(CU-ZN 합금), 청동 또는 S, Pb등 여러 금속 합금들이며, 시계, 안경, 장식품들의 형태를 나타내도록 형성하는데 적합한 재질이다.2A shows a cross section of the surface treatment layer obtained by the treatment method of the present invention. Material 1 is made of SUS and BSP (CU-ZN alloy), bronze or various metal alloys such as S and Pb, and is suitable for forming to form watches, glasses, and ornaments.

기부층 2는 고융점 금속 니켈(Ni), 크롬(Cr), 팔라듐(Pb), 로듐(Rh), 금(Au), 은(Ag)등의 도금막을 형성한 표면을 나타낸 것이다.The base layer 2 shows a surface on which a plating film of high melting point metal nickel (Ni), chromium (Cr), palladium (Pb), rhodium (Rh), gold (Au), silver (Ag), or the like is formed.

기부층 3은 은폐물을 코팅한 것이다. 기부층 4는 고진공도금을 형성시킨 표면이다.Base layer 3 is a coating of the concealment. Base layer 4 is a surface on which high vacuum plating is formed.

상기의 표면처리중에서, 기부층 3에서 피막보호수단으로 은폐물을 부분도포하고, 진공도금전 표면처리하는데 있어서 표면처리는 강산, 강알칼리 탈지제에 의해 표면탈지 및 용제에 의한 세척을 하고, 필요시 알칼리(-)전해탈지까지 하고 표면의 오물을 완전히 제거함으로써 수행한다. 만약 오물, 및 유분을 완전히 제거하지 않고 진공 도금할 경우 도금막층의 파괴로 인해 밀착력이 매우 불안정하다. 은폐물의 부분도포후의 표면처리는 진공도금에 미치는 영향이 크다.Among the surface treatments described above, the cover layer is partially covered by the protective film at the base layer 3, and in the surface treatment before vacuum plating, the surface treatment is performed by surface degreasing and solvent cleaning with strong acid and strong alkali degreasing agent, and alkali (-) if necessary. This is done by electrolytic degreasing and completely removing surface dirt. If vacuum plating is performed without completely removing dirt and oil, the adhesion is very unstable due to the destruction of the plating layer. Surface treatment after partial application of the concealment has a great effect on vacuum plating.

표면처리완료후 진공상태(고진공 10-6TORR)의 챔버내에 피도금체를 놓고 진공도금을 수행한다. 이때 이온플레이팅의 경우 금색에 가까운 색을 내기 위해서는 질화티탄(TiN), 질화탄탈륨(TaN)을 사용하며, 흑색에 가까운 색을 내기위해서는 탄화티탄, (TiC), 탄화탄탈륨(Tac), 산화크롬(Cr2O2Cr23O8, Cr23O8) 등을 사용하여 다양하게 응용할 수 있다.After completion of surface treatment, the plated body is placed in a vacuum chamber (high vacuum 10-6 TORR) and vacuum plating is performed. In the case of ion plating, titanium nitride (TiN) and tantalum nitride (TaN) are used to produce a color close to gold, and titanium carbide, (TiC), tantalum carbide (Tac), and chromium oxide are used to produce a color close to black. (Cr 2 O 2 Cr 23 O 8 , Cr 23 O 8 ) and the like can be used in various applications.

제2b도는 본 발명의 이중, 삼중, 진공부분도금 표면처리층의 단면을 보여준 것이다. 기부층 4까지 형성시킨후 은폐물의 박리를 행하면 은폐물 3과 은폐물 3상의 기부층 4가 박리되어 기부층 3밑의 기부층 2와 기부층 3이외의 부분의 기부층 4가 부분적으로 형성되어 있는 형상이 된다. 소재 1상의 기부층 2, 기부층 4, 기부층 5는 고진공 표면처리층으로서 색상이 다른 진공도금층의 형성을 표시하며, 기부층 2 및 기부층 4에 각각 은폐물을 부분도포하여 기부층 2, 기부층 4, 기부층 5가 부분적으로 나타나도록 한것이다.Figure 2b shows a cross section of the double, triple, vacuum partial plating surface treatment layer of the present invention. After the base layer 4 is formed, the concealment is peeled off, and the concealment 3 and the base layer 4 on the concealment 3 are peeled off, and the base layer 2 under the base layer 3 and the base layer 4 other than the base layer 3 are partially formed. Becomes Base layer 2, base layer 4, and base layer 5 on the material 1 indicate the formation of a vacuum plating layer having a different color as a high vacuum surface treatment layer, and partially cover the base layer 2 and the base layer 4, respectively, to partially cover the base layer 2, base. Layer 4 and base 5 are partially visible.

전자의 제2a도는 습식도금과 진공도금을 병합한 것이며, 제2b도는 진공도금을 여러차례 행하는 기법으로 표면처리하는 것을 나타낸 것이다. 제2b도에서 은폐물의 박리방법은 제2a도와 동일하다.Figure 2a of the former is a combination of wet plating and vacuum plating, and Figure 2b shows surface treatment by a technique of performing vacuum plating several times. The peeling method of the concealment in FIG. 2b is the same as that of FIG.

본 발명의 방법에 의해 수득한 진공도금막은 균일한 색상을 유지하였으며, 일반 외관은 고융점 소재를 사용하여 작업한 것과 차가 전혀 없으며 매우 우수하였다.The vacuum plated film obtained by the method of the present invention maintained a uniform color, and the general appearance was very different from that of working with a high melting point material and was very excellent.

본 발명의 방법에 의하여 수득된 제품에 대하여 여러가지 조건에 대해 신뢰성시험을 실시하였다. 시험조건과 그 결과는 다음과 같다.Reliability tests were conducted on various conditions for the products obtained by the method of the present invention. Test conditions and results are as follows.

시험조건 : 인공땀 : 40℃ ×24시간 반침적Test conditions: artificial sweat: 40 ℃ × 24 hours half deposition

식염수 : 40℃ ×12시간 반침적Saline: 40 ℃ × 12 hours, half deposition

밀착 : 90도 굽힘실험Close contact: 90 degree bending test

NH4OH : 4시간 폭기NH 4 OH: 4 hour aeration

열충격(H1S) : 200℃ ×20분후 자연냉각Thermal Shock (H 1 S): Natural Cooling after 200 ℃ × 20 minutes

Figure kpo00002
Figure kpo00002

상기의 시험결과에서도 알수 있는바와 같이 본 발명의 방법에 의해 수득된 도금제품을 인공땀, 식염수, 밀착, NH4OH 폭기, 열충격에 대해 모두 강한 내성을 나타내었다.As can be seen from the above test results, the plated products obtained by the method of the present invention showed strong resistance to artificial sweat, saline, adhesion, NH 4 OH aeration, and thermal shock.

Claims (10)

순금속 또는 금속 합금상에 니켈(Ni), 크롬(Cr), 카드뮴(Cd), 구리(Cu), 인듐(In), 코발트(Co) 및 그 합금의 전해 도금을 수행하고 은폐물로 부분도포한후, 진공도금을 실시하고 은폐물을 박리함을 특징으로 하는 2색을 나타내는 부분도금 방법.Electrolytic plating of nickel (Ni), chromium (Cr), cadmium (Cd), copper (Cu), indium (In), cobalt (Co) and their alloys on a pure metal or metal alloy, and then partially coated with a concealment The partial plating method showing two colors characterized by performing vacuum plating and peeling a concealed object. 제1항의 방법에 의해 부분도금된 물품.An article partially plated by the method of claim 1. 순금속 또는 금속합금상에 진공도금을 실시하고, 은폐물로 부분도포한 후, 니켈(Ni), 크롬(Cr), 팔라듐(Pd), 로듐(Rh), 금(Au), 은(Ag), 카드뮴(Cd), 구리(Cu), 인듐(In), 코발트(Co) 및 그 합금의 전해도금 및 무전해 도금을 실시하고 은폐물을 박리함을 특징으로 하는, 2색을 나타내는 부분도금 방법.Vacuum plating on pure metals or metal alloys, partially coated with concealed materials, and then nickel (Ni), chromium (Cr), palladium (Pd), rhodium (Rh), gold (Au), silver (Ag), cadmium (Cd), copper (Cu), indium (In), cobalt (Co) and their alloys are subjected to electroplating and electroless plating, and the concealment is peeled off. 제3항의 방법에 의해 부분도금된 물품.An article partially plated by the method of claim 3. 제1항 및 제3항의 방법에 따라 진공도금 또는 전해도금 또는 무전해 도금을 중복실시하고 은폐물을 박리함을 특징으로하는, 3색을 나타내는 부분도금 방법.A partial plating method of three colors, characterized in that the vacuum plating or electroplating or electroless plating is carried out in accordance with the method of claims 1 and 3, and the concealment is peeled off. 제5항의 방법에 의해 부분도금된 물품.An article partially plated by the method of claim 5. 순금속 또는 금속합금상에 Ti, Tin, TiCN 막층을 진공도금으로 형성하고, 이 상부에 은폐물을 부분도포한후 다시 진공도금을 실시하고 은폐물을 박리함을 특징으로 하는 2색을 나타내는 부분도금 방법.A partial plating method of two colors, characterized by forming a Ti, Tin, TiCN film layer on a pure metal or a metal alloy by vacuum plating, partially applying a concealment on the upper part, and then vacuum plating and peeling off the concealment. 제7항의 방법에 의해 부분도금된 물품.An article partially plated by the method of claim 7. 제7항의 방법에 따라 진공도금, 은폐물도포를 중복실시하고 은폐물을 박리함을 특징으로 하는 3색을 나타내는 부분도금방법.A partial plating method of three colors, characterized in that the vacuum plating, the coating of the concealed substance is repeated according to the method of claim 7, and the concealed substance is peeled off. 제9항의 방법에 따라 부분도금된 물품.Partially plated according to the method of claim 9.
KR1019890019870A 1989-12-28 1989-12-28 Coating method on selected surface areas by a vacuum evaporation KR920002411B1 (en)

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